Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _audit_creation_method 'SHELXL-97 plus manual edit of cif file' _journal_coden_Cambridge 0222 _publ_section_title ; Synthesis and characterisation of N-coordinated pentafluorophenyl gold(I) thiazole-derived complexes and an unusual self-assembly to form a tetrameric gold(I) complex ; _publ_contact_author_name 'Dr. Stephanie Cronje' _publ_contact_author_address ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_phone '+27 21 808 2180' _publ_contact_author_fax '+27 21 808 3360' _publ_contact_author_email scron@sun.ac.za loop_ _publ_author_name _publ_author_address S.Cronje ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; H.G.Raubenheimer ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; H.S.C.Spies ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; C.Esterhuysen ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; ; H.Schmidbaur ; ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching Germany ; A.Schier ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching Germany ; G.J.Kruger ; Department of Chemistry and Biochemistry Rand Afrikaans University P O Box 524 Auckland Park, Johannesburg 2006 South Africa ; _publ_section_references ; Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838 Hall, S.R., King, G.S.D. & Stewart, J.M. (1995). Eds. Xtal3.4 Reference Manual. University of Western Australia: Lamb, Perth. Nonius BV (1998) COLLECT. Data collection software. Delft, The Netherlands. North, A. C. T., Phillips D. C. & Mathews, F. S. (1968). Acta. Cryst. A24, 351-359. Otwinowski, Z. & Minor, W. (1997) Methods Enzymol., 276, 307. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of Gottingen, Germany. ; data_2 _database_code_CSD 207317 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4-methylthiazole-\kN)pentafluorophenylgold(I) ; _chemical_name_common (4-methylthiazole-kappaN)pentafluorophenylgold(i) _chemical_melting_point '58\% decomposed' _chemical_formula_moiety 'C10 H5 Au F5 N S' _chemical_formula_sum 'C10 H5 Au F5 N S' _chemical_formula_weight 463.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 7.5140(15) _cell_length_b 21.352(3) _cell_length_c 8.1590(13) _cell_angle_alpha 90.00 _cell_angle_beta 115.528(17) _cell_angle_gamma 90.00 _cell_volume 1181.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 2 _cell_measurement_theta_max 17 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 12.674 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.14 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4F' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3443 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3443 _reflns_number_gt 2521 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction 'CAD-4 Software' _computing_structure_solution 'Xtal (Hall et al., 1995)' _computing_structure_refinement 'Xtal (Hall et al., 1995)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material Xtal _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details '??calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2521 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_ref 0.039 _refine_ls_wR_factor_gt 0.043 _refine_ls_goodness_of_fit_ref 2.618 _refine_ls_restrained_S_all 2.618 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.45113(7) 0.52754(2) 0.66815(7) 0.0504(2) Uani 1 1 d . . . S1 S 0.0592(6) 0.6677(2) 0.2562(5) 0.081(2) Uani 1 1 d . . . N1 N 0.314(2) 0.6022(4) 0.496(1) 0.056(5) Uani 1 1 d . . . C1 C 0.138(2) 0.5994(5) 0.373(2) 0.066(7) Uani 1 1 d . . . C2 C 0.279(2) 0.7021(5) 0.394(2) 0.070(7) Uani 1 1 d . . . C3 C 0.400(2) 0.6624(5) 0.513(2) 0.058(6) Uani 1 1 d . . . C4 C 0.600(2) 0.6727(5) 0.653(2) 0.09(1) Uani 1 1 d . . . C5 C 0.583(2) 0.4614(5) 0.855(1) 0.051(5) Uani 1 1 d . . . C6 C 0.751(2) 0.4714(5) 0.995(2) 0.053(5) Uani 1 1 d . . . C7 C 0.854(2) 0.4291(5) 1.133(2) 0.061(6) Uani 1 1 d . . . C8 C 0.772(2) 0.3690(5) 1.116(2) 0.064(7) Uani 1 1 d . . . C9 C 0.605(2) 0.3556(5) 0.970(2) 0.061(7) Uani 1 1 d . . . C10 C 0.512(2) 0.4002(5) 0.843(2) 0.054(6) Uani 1 1 d . . . F1 F 0.835(1) 0.5299(3) 1.027(1) 0.070(3) Uani 1 1 d . . . F2 F 1.022(1) 0.4438(3) 1.284(1) 0.085(4) Uani 1 1 d . . . F3 F 0.869(1) 0.3261(3) 1.246(1) 0.092(5) Uani 1 1 d . . . F4 F 0.530(1) 0.2966(3) 0.954(1) 0.099(5) Uani 1 1 d . . . F5 F 0.342(1) 0.3825(3) 0.705(1) 0.084(4) Uani 1 1 d . . . H1 H .06127 .56437 .34641 .08000 Uiso 1 1 d . . . H2 H .30683 .74327 .38339 .08000 Uiso 1 1 d . . . H41 H .69043 .64244 .65036 .08000 Uiso 1 1 d . . . H42 H .60047 .67031 .77593 .08000 Uiso 1 1 d . . . H43 H .64246 .71414 .64245 .08000 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au .0540(3) .0465(2) .0535(3) .0021(3) .0259(2) -.0046(2) S1 .076(3) .078(2) .093(3) .025(2) .041(2) .022(2) N1 .071(8) .061(6) .034(5) .005(5) .021(5) .000(5) C1 .07(1) .061(7) .059(9) .004(7) .020(8) .009(6) C2 .08(1) .050(7) .09(1) .012(7) .047(9) .015(7) C3 .07(1) .053(7) .066(9) -.014(7) .046(8) -.016(6) C4 .09(1) .060(8) .15(2) -.018(8) .06(1) -.008(9) C5 .061(8) .060(7) .026(6) .008(6) .013(6) -.002(5) C6 .061(8) .042(5) .056(7) .001(6) .027(6) -.002(6) C7 .065(9) .050(7) .067(9) .001(6) .028(8) -.008(6) C8 .08(1) .051(7) .068(9) .019(7) .037(8) .016(7) C9 .08(1) .042(6) .08(1) -.008(6) .046(9) -.010(6) C10 .057(9) .064(7) .048(7) -.014(6) .030(7) -.007(6) F1 .071(5) .048(3) .080(5) -.010(4) .023(4) .006(4) F2 .080(6) .072(4) .072(6) .011(4) .006(5) .010(4) F3 .120(7) .065(4) .096(6) .019(4) .051(6) .025(4) F4 .141(8) .047(4) .123(7) -.028(4) .071(6) -.009(4) F5 .081(6) .075(5) .097(6) -.029(4) .040(5) -.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au N1 2.081(8) . ? Au C5 2.00(1) . ? S1 C1 1.70(1) . ? S1 C2 1.71(1) . ? N1 C1 1.27(1) . ? N1 C3 1.42(1) . ? C1 H1 .91(1) . ? C2 C3 1.32(2) . ? C2 H2 .92(1) . ? C3 C4 1.46(2) . ? C4 H41 .95(2) . ? C4 H42 1.00(2) . ? C4 H43 .96(1) . ? C5 C6 1.31(1) . ? C5 C10 1.40(2) . ? C6 C7 1.39(2) . ? C6 F1 1.37(1) . ? C7 C8 1.40(2) . ? C7 F2 1.37(1) . ? C8 C9 1.34(2) . ? C8 F3 1.35(1) . ? C9 C10 1.36(2) . ? C9 F4 1.36(1) . ? C10 F5 1.34(1) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Au C5 174.0(4) . . ? C1 S1 C2 89.7(6) . . ? Au N1 C1 122.6(8) . . ? Au N1 C3 123.7(7) . . ? C1 N1 C3 113.5(9) . . ? S1 C1 N1 113.1(9) . . ? S1 C1 H1 122(1) . . ? N1 C1 H1 124(1) . . ? S1 C2 C3 112.0(9) . . ? S1 C2 H2 123(1) . . ? C3 C2 H2 125(1) . . ? N1 C3 C2 112(1) . . ? N1 C3 C4 119(1) . . ? C2 C3 C4 129(1) . . ? C3 C4 H41 113(1) . . ? C3 C4 H42 109(2) . . ? C3 C4 H43 110(1) . . ? H41 C4 H42 107(1) . . ? H41 C4 H43 111(2) . . ? H42 C4 H43 106(1) . . ? Au C5 C6 121.8(8) . . ? Au C5 C10 124.1(7) . . ? C6 C5 C10 114.0(9) . . ? C5 C6 C7 127(1) . . ? C5 C6 F1 120.3(9) . . ? C7 C6 F1 112.9(9) . . ? C6 C7 C8 116(1) . . ? C6 C7 F2 124(1) . . ? C8 C7 F2 120(1) . . ? C7 C8 C9 119(1) . . ? C7 C8 F3 118(1) . . ? C9 C8 F3 122(1) . . ? C8 C9 C10 120(1) . . ? C8 C9 F4 118(1) . . ? C10 C9 F4 121(1) . . ? C5 C10 C9 123(1) . . ? C5 C10 F5 121.0(9) . . ? C9 C10 F5 116(1) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.410 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.060 #===END data_5 _database_code_CSD 207318 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4-methyl-3H-thiazole-2-thione-\kS)pentafluorophenylgold(I) ; _chemical_name_common (4-methyl-3H-thiazole-2-thione-kappaS)pentafluorophenylgold(i) _chemical_melting_point '90\% decomposed' _chemical_formula_moiety 'C10 H5 Au F5 N S2' _chemical_formula_sum 'C10 H5 Au F5 N S2' _chemical_formula_weight 495.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 7.4858(5) _cell_length_b 12.2944(9) _cell_length_c 13.5153(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.933(2) _cell_angle_gamma 90.00 _cell_volume 1242.23(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1982 _cell_measurement_theta_min 1 _cell_measurement_theta_max 24.71 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 12.223 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.01 _exptl_absorpt_correction_T_max 0.16 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 3901 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.44 _reflns_number_total 2203 _reflns_number_gt 1846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+11.0960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2201 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.36682(7) 0.51414(5) 0.63145(4) 0.0589(3) Uani 1 1 d . . . S1 S 0.2422(6) 0.4270(3) 0.4937(3) 0.0635(10) Uani 1 1 d . . . S2 S 0.2311(6) 0.6654(3) 0.4405(3) 0.0686(11) Uani 1 1 d . . . C1 C 0.1858(18) 0.5317(11) 0.4177(11) 0.050(3) Uani 1 1 d . . . C6 C 0.557(2) 0.5297(13) 0.8322(13) 0.066(4) Uani 1 1 d . . . C10 C 0.488(2) 0.6998(13) 0.7639(10) 0.059(4) Uani 1 1 d . . . C7 C 0.636(2) 0.5790(14) 0.9165(11) 0.068(4) Uani 1 1 d . . . C5 C 0.4809(18) 0.5888(12) 0.7554(10) 0.054(3) Uani 1 1 d . . . C8 C 0.640(2) 0.6888(17) 0.9235(12) 0.072(4) Uani 1 1 d . . . N1 N 0.1022(17) 0.5243(9) 0.3262(10) 0.055(3) Uani 1 1 d . . . H1 H 0.0753 0.4626 0.2995 0.066 Uiso 1 1 calc R . . C3 C 0.064(2) 0.6193(13) 0.2798(12) 0.061(4) Uani 1 1 d . . . C4 C -0.028(2) 0.6179(15) 0.1812(10) 0.072(4) Uani 1 1 d . . . H4A H -0.0403 0.6911 0.1569 0.108 Uiso 1 1 calc R . . H4B H -0.1437 0.5856 0.1853 0.108 Uiso 1 1 calc R . . H4C H 0.0414 0.5762 0.1367 0.108 Uiso 1 1 calc R . . C9 C 0.567(2) 0.7496(14) 0.8451(12) 0.066(4) Uani 1 1 d . . . C2 C 0.127(2) 0.7025(13) 0.3281(13) 0.069(4) Uani 1 1 d . . . H2 H 0.1169 0.7738 0.3053 0.083 Uiso 1 1 calc R . . F1 F 0.5558(15) 0.4207(8) 0.8316(8) 0.083(3) Uani 1 1 d . . . F5 F 0.4159(16) 0.7649(8) 0.6930(8) 0.090(3) Uani 1 1 d . . . F2 F 0.7098(18) 0.5177(9) 0.9884(8) 0.093(3) Uani 1 1 d . . . F4 F 0.5636(16) 0.8601(8) 0.8495(8) 0.091(3) Uani 1 1 d . . . F3 F 0.7151(16) 0.7407(10) 1.0016(7) 0.099(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0624(4) 0.0626(4) 0.0511(4) 0.0048(2) -0.0045(3) 0.0013(2) S1 0.080(3) 0.051(2) 0.058(2) 0.0046(16) -0.0106(18) -0.0007(16) S2 0.085(3) 0.0475(19) 0.071(3) -0.0018(17) -0.016(2) -0.0049(17) C1 0.051(7) 0.044(7) 0.055(8) -0.003(6) -0.003(6) 0.002(5) C6 0.081(11) 0.062(9) 0.054(9) 0.003(7) 0.004(8) 0.004(8) C10 0.060(8) 0.083(10) 0.031(7) 0.009(6) -0.007(6) 0.004(7) C7 0.092(12) 0.072(10) 0.040(8) 0.015(7) 0.003(7) 0.015(8) C5 0.054(8) 0.061(8) 0.045(8) 0.006(6) -0.010(6) 0.002(6) C8 0.064(9) 0.104(13) 0.047(9) -0.007(8) -0.008(7) -0.003(8) N1 0.058(7) 0.049(6) 0.056(7) -0.001(5) -0.004(5) -0.003(5) C3 0.065(9) 0.059(9) 0.059(9) 0.011(7) 0.006(7) -0.002(6) C4 0.091(12) 0.085(11) 0.039(8) 0.021(7) -0.017(7) 0.006(8) C9 0.068(9) 0.071(10) 0.059(9) -0.003(7) -0.010(7) 0.004(7) C2 0.086(11) 0.049(8) 0.071(11) 0.010(8) -0.010(8) 0.004(7) F1 0.106(8) 0.061(6) 0.079(7) 0.013(5) -0.014(6) 0.014(5) F5 0.116(9) 0.069(6) 0.084(7) 0.022(5) -0.011(6) 0.021(5) F2 0.117(9) 0.098(8) 0.062(7) 0.016(5) -0.021(6) 0.019(6) F4 0.112(8) 0.068(6) 0.091(7) -0.002(5) -0.021(6) -0.002(6) F3 0.107(9) 0.111(9) 0.074(7) -0.009(6) -0.023(6) -0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au C5 2.057(14) . ? Au S1 2.304(4) . ? S1 C1 1.686(15) . ? S2 C1 1.704(13) . ? S2 C2 1.734(17) . ? C1 N1 1.36(2) . ? C6 F1 1.340(19) . ? C6 C5 1.37(2) . ? C6 C7 1.40(3) . ? C10 F5 1.341(16) . ? C10 C9 1.36(2) . ? C10 C5 1.37(2) . ? C7 F2 1.328(18) . ? C7 C8 1.35(3) . ? C8 F3 1.333(18) . ? C8 C9 1.39(2) . ? N1 C3 1.349(19) . ? N1 H1 0.8600 . ? C3 C2 1.29(2) . ? C3 C4 1.47(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C9 F4 1.360(19) . ? C2 H2 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Au S1 178.7(4) . . ? C1 S1 Au 102.5(5) . . ? C1 S2 C2 91.1(8) . . ? N1 C1 S1 126.3(10) . . ? N1 C1 S2 107.8(10) . . ? S1 C1 S2 125.8(9) . . ? F1 C6 C5 121.7(15) . . ? F1 C6 C7 116.2(14) . . ? C5 C6 C7 122.1(15) . . ? F5 C10 C9 116.7(15) . . ? F5 C10 C5 121.4(13) . . ? C9 C10 C5 121.9(13) . . ? F2 C7 C8 120.4(16) . . ? F2 C7 C6 119.7(15) . . ? C8 C7 C6 119.9(15) . . ? C6 C5 C10 116.9(14) . . ? C6 C5 Au 121.4(12) . . ? C10 C5 Au 121.7(10) . . ? F3 C8 C7 122.7(16) . . ? F3 C8 C9 118.8(17) . . ? C7 C8 C9 118.5(15) . . ? C3 N1 C1 116.3(12) . . ? C3 N1 H1 121.9 . . ? C1 N1 H1 121.9 . . ? C2 C3 N1 112.8(14) . . ? C2 C3 C4 127.5(15) . . ? N1 C3 C4 119.4(15) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? F4 C9 C10 118.5(15) . . ? F4 C9 C8 120.8(15) . . ? C10 C9 C8 120.7(16) . . ? C3 C2 S2 111.8(12) . . ? C3 C2 H2 124.1 . . ? S2 C2 H2 124.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F1 0.86 2.43 3.203(15) 149.1 2_546 N1 H1 F2 0.86 2.55 3.310(17) 147.7 2_546 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.412 _refine_diff_density_min -2.439 _refine_diff_density_rms 0.280 #===END data_6 _database_code_CSD 207319 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis[(\m4-methyl-3H-thiazole-2-thionate-\kN,S)gold(I)] ; _chemical_name_common tetrakis((mu4-methyl-3H-thiazole-2-thionate-kappaN,S)gold(i)) _chemical_melting_point '128\% decomposed' _chemical_formula_moiety '2(C16 H16 Au4 N4 S8)' _chemical_formula_sum 'C32 H32 Au8 N8 S16' _chemical_formula_weight 2617.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6203(2) _cell_length_b 14.5242(2) _cell_length_c 16.0147(2) _cell_angle_alpha 88.2480(10) _cell_angle_beta 89.3080(10) _cell_angle_gamma 81.5490(10) _cell_volume 2672.21(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10945 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.2 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 22.532 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.002 _exptl_absorpt_correction_T_max 0.043 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 15382 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9408 _reflns_number_gt 7405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+8.1687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9408 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1518 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C111 C 0.1797(13) 1.1619(10) -0.0253(9) 0.032(3) Uani 1 1 d . . . C113 C 0.1288(15) 1.3146(12) -0.0596(11) 0.044(4) Uani 1 1 d . . . C112 C 0.0593(17) 1.2777(13) -0.1122(12) 0.059(6) Uani 1 1 d . . . H112 H 0.0077 1.3133 -0.1505 0.070 Uiso 1 1 calc R . . C114 C 0.1405(16) 1.4142(10) -0.0510(11) 0.045(4) Uani 1 1 d . . . H11A H 0.1111 1.4494 -0.1014 0.067 Uiso 1 1 calc R . . H11B H 0.2226 1.4202 -0.0435 0.067 Uiso 1 1 calc R . . H11C H 0.0955 1.4387 -0.0023 0.067 Uiso 1 1 calc R . . C121 C 0.3907(15) 1.0889(11) 0.3197(13) 0.049(5) Uani 1 1 d . . . C123 C 0.5557(15) 1.0742(13) 0.2454(12) 0.053(5) Uani 1 1 d . . . C122 C 0.5999(17) 1.0660(15) 0.3220(15) 0.068(6) Uani 1 1 d . . . H122 H 0.6808 1.0558 0.3340 0.082 Uiso 1 1 calc R . . C124 C 0.6263(17) 1.0682(16) 0.1667(14) 0.073(7) Uani 1 1 d . . . H12A H 0.7067 1.0412 0.1794 0.110 Uiso 1 1 calc R . . H12B H 0.6251 1.1308 0.1416 0.110 Uiso 1 1 calc R . . H12C H 0.5935 1.0289 0.1274 0.110 Uiso 1 1 calc R . . C131 C -0.0137(14) 1.3207(11) 0.1442(10) 0.037(4) Uani 1 1 d . . . C133 C -0.0598(16) 1.1757(12) 0.1195(11) 0.048(5) Uani 1 1 d . . . C132 C -0.1463(15) 1.2308(13) 0.0750(12) 0.050(5) Uani 1 1 d . . . H132 H -0.2053 1.2075 0.0449 0.060 Uiso 1 1 calc R . . C134 C -0.041(2) 1.0725(13) 0.1290(16) 0.079(7) Uani 1 1 d . . . H13A H -0.1021 1.0471 0.1000 0.119 Uiso 1 1 calc R . . H13B H -0.0422 1.0546 0.1885 0.119 Uiso 1 1 calc R . . H13C H 0.0352 1.0478 0.1050 0.119 Uiso 1 1 calc R . . C141 C 0.4972(14) 1.3211(11) 0.2093(9) 0.036(4) Uani 1 1 d . . . C143 C 0.4314(18) 1.3296(12) 0.3434(12) 0.052(5) Uani 1 1 d . . . C142 C 0.549(2) 1.3187(16) 0.3565(14) 0.079(7) Uani 1 1 d . . . H142 H 0.5840 1.3151 0.4101 0.095 Uiso 1 1 calc R . . C144 C 0.3387(18) 1.3425(18) 0.4088(15) 0.082(8) Uani 1 1 d . . . H14A H 0.3693 1.3135 0.4616 0.123 Uiso 1 1 calc R . . H14B H 0.2723 1.3133 0.3916 0.123 Uiso 1 1 calc R . . H14C H 0.3136 1.4092 0.4164 0.123 Uiso 1 1 calc R . . C211 C -0.0008(15) 0.6836(11) 0.3713(10) 0.042(4) Uani 1 1 d . . . C213 C -0.0507(15) 0.8387(12) 0.3918(11) 0.045(4) Uani 1 1 d . . . C212 C -0.1190(15) 0.7993(15) 0.4491(13) 0.060(5) Uani 1 1 d . . . H212 H -0.1711 0.8351 0.4859 0.072 Uiso 1 1 calc R . . C214 C -0.043(2) 0.9397(13) 0.3743(18) 0.086(8) Uani 1 1 d . . . H21A H -0.1009 0.9646 0.3322 0.129 Uiso 1 1 calc R . . H21B H 0.0349 0.9462 0.3534 0.129 Uiso 1 1 calc R . . H21C H -0.0586 0.9742 0.4258 0.129 Uiso 1 1 calc R . . C241 C 0.3827(15) 0.8349(10) 0.1790(12) 0.043(4) Uani 1 1 d . . . C243 C 0.5510(15) 0.8218(12) 0.2517(15) 0.059(6) Uani 1 1 d . . . C242 C 0.5947(18) 0.8246(17) 0.1749(14) 0.075(7) Uani 1 1 d . . . H242 H 0.6754 0.8207 0.1625 0.090 Uiso 1 1 calc R . . C244 C 0.6175(19) 0.8113(19) 0.3369(17) 0.092(9) Uani 1 1 d . . . H24A H 0.6059 0.7525 0.3651 0.139 Uiso 1 1 calc R . . H24B H 0.5875 0.8634 0.3724 0.139 Uiso 1 1 calc R . . H24C H 0.7007 0.8115 0.3264 0.139 Uiso 1 1 calc R . . C231 C 0.1914(14) 0.7939(11) 0.5301(10) 0.039(4) Uani 1 1 d . . . C232 C 0.0912(16) 0.6981(13) 0.6255(11) 0.053(5) Uani 1 1 d . . . H232 H 0.0460 0.6719 0.6672 0.064 Uiso 1 1 calc R . . C233 C 0.1560(16) 0.6469(12) 0.5700(11) 0.048(4) Uani 1 1 d . . . C234 C 0.1739(18) 0.5460(12) 0.5621(14) 0.062(6) Uani 1 1 d . . . H23A H 0.1244 0.5182 0.6026 0.094 Uiso 1 1 calc R . . H23B H 0.2557 0.5214 0.5728 0.094 Uiso 1 1 calc R . . H23C H 0.1537 0.5307 0.5054 0.094 Uiso 1 1 calc R . . C221 C 0.4972(15) 0.5790(11) 0.2719(10) 0.040(4) Uani 1 1 d . . . C222 C 0.534(2) 0.5725(15) 0.1234(13) 0.069(6) Uani 1 1 d . . . H222 H 0.5635 0.5694 0.0679 0.083 Uiso 1 1 calc R . . C223 C 0.4191(15) 0.5792(11) 0.1433(12) 0.045(4) Uani 1 1 d . . . C224 C 0.3269(18) 0.5821(14) 0.0831(11) 0.059(5) Uani 1 1 d . . . H22A H 0.3435 0.6207 0.0344 0.089 Uiso 1 1 calc R . . H22B H 0.2529 0.6088 0.1086 0.089 Uiso 1 1 calc R . . H22C H 0.3219 0.5188 0.0655 0.089 Uiso 1 1 calc R . . Au11 Au 0.34024(5) 1.08631(4) 0.13542(4) 0.03537(17) Uani 1 1 d . . . Au12 Au 0.13928(5) 1.16928(4) 0.24051(4) 0.03636(17) Uani 1 1 d . . . Au13 Au 0.23435(5) 1.35695(4) 0.21902(4) 0.03502(17) Uani 1 1 d . . . Au14 Au 0.33557(5) 1.27871(4) 0.05770(4) 0.03349(17) Uani 1 1 d . . . Au21 Au 0.23536(5) 0.58936(4) 0.27913(4) 0.03772(17) Uani 1 1 d . . . Au24 Au 0.13888(6) 0.79791(5) 0.25935(4) 0.03982(18) Uani 1 1 d . . . Au23 Au 0.33438(6) 0.84173(5) 0.36302(4) 0.03917(18) Uani 1 1 d . . . Au22 Au 0.34310(5) 0.64709(4) 0.43492(4) 0.03780(17) Uani 1 1 d . . . N11 N 0.1985(12) 1.2464(8) -0.0114(8) 0.037(3) Uani 1 1 d . . . N13 N 0.0130(11) 1.2295(9) 0.1577(8) 0.035(3) Uani 1 1 d . . . N14 N 0.4046(11) 1.3312(9) 0.2583(8) 0.037(3) Uani 1 1 d . . . N21 N 0.0214(11) 0.7682(9) 0.3470(8) 0.037(3) Uani 1 1 d . . . N24 N 0.4287(12) 0.8281(8) 0.2548(8) 0.040(3) Uani 1 1 d . . . N23 N 0.2121(10) 0.7055(9) 0.5154(8) 0.035(3) Uani 1 1 d . . . N22 N 0.3974(11) 0.5842(9) 0.2265(9) 0.039(3) Uani 1 1 d . . . N12 N 0.4364(13) 1.0844(9) 0.2437(8) 0.040(3) Uani 1 1 d . . . S111 S 0.2471(5) 1.0582(3) 0.0179(3) 0.0506(12) Uani 1 1 d . . . S112 S 0.0752(5) 1.1595(3) -0.1013(3) 0.0576(13) Uani 1 1 d . . . S121 S 0.2440(4) 1.0977(3) 0.3480(3) 0.0496(11) Uani 1 1 d . . . S122 S 0.4910(5) 1.0763(4) 0.3966(3) 0.0664(15) Uani 1 1 d . . . S131 S 0.0484(4) 1.4096(3) 0.1833(3) 0.0420(10) Uani 1 1 d . . . S132 S -0.1336(5) 1.3464(4) 0.0809(4) 0.0641(15) Uani 1 1 d . . . S141 S 0.5042(4) 1.3190(3) 0.1027(3) 0.0473(11) Uani 1 1 d . . . S142 S 0.6251(4) 1.3122(4) 0.2639(4) 0.0651(15) Uani 1 1 d . . . S211 S 0.0567(4) 0.5781(3) 0.3304(3) 0.0536(12) Uani 1 1 d . . . S212 S -0.1035(4) 0.6859(4) 0.4487(3) 0.0619(13) Uani 1 1 d . . . S241 S 0.2410(5) 0.8437(4) 0.1482(3) 0.0564(13) Uani 1 1 d . . . S242 S 0.4867(5) 0.8364(4) 0.0997(3) 0.0706(16) Uani 1 1 d . . . S231 S 0.2409(5) 0.8868(3) 0.4831(3) 0.0529(12) Uani 1 1 d . . . S232 S 0.0960(4) 0.8148(3) 0.6153(3) 0.0525(12) Uani 1 1 d . . . S221 S 0.5115(4) 0.5761(4) 0.3793(3) 0.0570(13) Uani 1 1 d . . . S222 S 0.6179(4) 0.5702(4) 0.2089(4) 0.0670(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C111 0.040(9) 0.038(8) 0.019(8) -0.007(6) 0.008(6) -0.010(7) C113 0.039(9) 0.049(10) 0.041(11) 0.005(8) -0.006(8) 0.004(8) C112 0.067(13) 0.055(11) 0.050(12) -0.008(9) -0.026(10) 0.010(10) C114 0.062(12) 0.023(8) 0.046(11) -0.008(7) -0.012(9) 0.006(7) C121 0.043(10) 0.033(9) 0.072(15) 0.008(9) -0.026(10) -0.004(8) C123 0.035(10) 0.060(12) 0.055(13) 0.002(9) -0.007(9) 0.019(9) C122 0.039(11) 0.077(14) 0.083(17) 0.006(12) -0.014(11) 0.005(10) C124 0.043(12) 0.091(16) 0.076(16) 0.001(12) 0.028(11) 0.018(11) C131 0.038(9) 0.039(9) 0.030(9) -0.003(7) -0.009(7) 0.002(7) C133 0.056(11) 0.055(11) 0.039(11) -0.004(8) -0.003(9) -0.023(9) C132 0.035(9) 0.064(12) 0.054(12) 0.003(9) -0.003(8) -0.017(9) C134 0.103(19) 0.051(12) 0.094(18) 0.007(11) -0.009(15) -0.045(13) C141 0.049(10) 0.046(9) 0.016(8) -0.006(7) -0.001(7) -0.011(8) C143 0.076(14) 0.041(10) 0.042(11) 0.011(8) -0.026(10) -0.013(9) C142 0.090(17) 0.100(17) 0.045(13) -0.005(12) -0.048(13) 0.000(14) C144 0.046(12) 0.12(2) 0.079(18) 0.039(15) -0.001(12) -0.020(13) C211 0.053(10) 0.047(10) 0.032(9) -0.017(7) 0.005(8) -0.026(8) C213 0.041(10) 0.047(10) 0.043(11) -0.007(8) -0.007(8) 0.005(8) C212 0.027(9) 0.085(15) 0.066(14) -0.027(11) 0.011(9) -0.002(9) C214 0.078(16) 0.040(11) 0.14(2) -0.026(13) -0.010(16) 0.008(11) C241 0.049(10) 0.022(8) 0.058(12) -0.001(7) 0.029(9) -0.008(7) C243 0.035(10) 0.042(10) 0.103(18) -0.012(10) 0.016(11) -0.019(8) C242 0.046(12) 0.110(19) 0.069(16) -0.007(13) 0.040(11) -0.016(12) C244 0.050(13) 0.12(2) 0.10(2) 0.035(17) 0.009(13) -0.012(14) C231 0.037(9) 0.040(9) 0.039(10) -0.010(7) 0.007(7) -0.001(7) C232 0.052(11) 0.071(13) 0.037(11) -0.012(9) 0.027(9) -0.009(10) C233 0.054(11) 0.047(10) 0.043(11) -0.002(8) 0.005(9) -0.009(9) C234 0.070(14) 0.043(11) 0.073(15) 0.013(10) 0.025(11) -0.011(10) C221 0.048(10) 0.042(9) 0.028(9) -0.017(7) 0.015(8) -0.002(8) C222 0.092(17) 0.071(14) 0.044(12) -0.008(10) 0.009(12) -0.014(12) C223 0.047(10) 0.039(9) 0.052(12) -0.012(8) 0.019(9) -0.012(8) C224 0.079(14) 0.077(14) 0.025(10) 0.021(9) 0.007(9) -0.025(11) Au11 0.0413(4) 0.0358(3) 0.0273(3) 0.0000(2) 0.0035(3) -0.0007(3) Au12 0.0342(3) 0.0379(3) 0.0358(4) 0.0001(3) 0.0067(3) -0.0019(3) Au13 0.0357(3) 0.0407(3) 0.0298(4) -0.0019(3) -0.0018(3) -0.0089(3) Au14 0.0381(3) 0.0367(3) 0.0263(3) -0.0030(2) -0.0012(3) -0.0070(3) Au21 0.0369(3) 0.0427(4) 0.0333(4) -0.0074(3) 0.0088(3) -0.0043(3) Au24 0.0389(4) 0.0460(4) 0.0357(4) -0.0028(3) 0.0025(3) -0.0100(3) Au23 0.0442(4) 0.0479(4) 0.0276(4) -0.0013(3) 0.0074(3) -0.0146(3) Au22 0.0380(4) 0.0471(4) 0.0279(4) -0.0074(3) 0.0073(3) -0.0042(3) N11 0.053(8) 0.034(7) 0.029(7) 0.000(6) 0.004(6) -0.020(6) N13 0.031(7) 0.046(8) 0.028(7) -0.010(6) 0.001(6) -0.002(6) N14 0.041(8) 0.048(8) 0.024(7) -0.007(6) -0.008(6) -0.011(6) N21 0.030(7) 0.050(8) 0.033(8) -0.011(6) 0.003(6) -0.009(6) N24 0.055(9) 0.033(7) 0.031(8) 0.009(6) 0.020(7) -0.009(6) N23 0.026(6) 0.051(8) 0.029(7) -0.011(6) 0.015(5) -0.005(6) N22 0.036(7) 0.033(7) 0.046(9) -0.010(6) 0.020(6) 0.004(6) N12 0.058(9) 0.038(7) 0.021(7) 0.003(6) 0.004(6) 0.001(6) S111 0.074(3) 0.036(2) 0.042(3) -0.0036(19) -0.010(2) -0.007(2) S112 0.060(3) 0.054(3) 0.062(3) -0.010(2) -0.024(3) -0.014(2) S121 0.053(3) 0.058(3) 0.034(3) 0.013(2) 0.010(2) 0.004(2) S122 0.066(3) 0.089(4) 0.039(3) -0.002(3) -0.015(3) 0.006(3) S131 0.043(2) 0.034(2) 0.049(3) -0.0061(18) -0.008(2) -0.0025(18) S132 0.054(3) 0.058(3) 0.082(4) 0.013(3) -0.034(3) -0.012(2) S141 0.040(2) 0.065(3) 0.039(3) -0.003(2) 0.0048(19) -0.018(2) S142 0.041(3) 0.092(4) 0.062(4) -0.013(3) -0.014(2) -0.006(3) S211 0.044(3) 0.054(3) 0.066(3) -0.019(2) 0.025(2) -0.015(2) S212 0.052(3) 0.074(3) 0.059(3) -0.006(3) 0.028(2) -0.009(3) S241 0.071(3) 0.067(3) 0.033(3) 0.010(2) 0.001(2) -0.021(3) S242 0.081(4) 0.084(4) 0.047(3) 0.001(3) 0.039(3) -0.017(3) S231 0.073(3) 0.050(3) 0.038(3) -0.009(2) 0.022(2) -0.018(2) S232 0.064(3) 0.053(3) 0.037(3) -0.008(2) 0.028(2) 0.001(2) S221 0.040(2) 0.086(4) 0.040(3) -0.014(2) 0.004(2) 0.009(2) S222 0.047(3) 0.092(4) 0.062(4) -0.014(3) 0.022(2) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C111 N11 1.305(18) . ? C111 S111 1.721(16) . ? C111 S112 1.734(15) . ? C113 C112 1.35(2) . ? C113 N11 1.402(19) . ? C113 C114 1.48(2) . ? C112 S112 1.704(19) . ? C112 H112 0.9500 . ? C114 H11A 0.9800 . ? C114 H11B 0.9800 . ? C114 H11C 0.9800 . ? C121 N12 1.32(2) . ? C121 S122 1.693(17) . ? C121 S121 1.75(2) . ? C123 C122 1.33(3) . ? C123 N12 1.37(2) . ? C123 C124 1.49(3) . ? C122 S122 1.72(2) . ? C122 H122 0.9500 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? C131 N13 1.33(2) . ? C131 S131 1.708(16) . ? C131 S132 1.722(15) . ? C133 C132 1.38(2) . ? C133 N13 1.39(2) . ? C133 C134 1.49(3) . ? C132 S132 1.713(19) . ? C132 H132 0.9500 . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C141 N14 1.32(2) . ? C141 S141 1.710(15) . ? C141 S142 1.720(16) . ? C143 C142 1.37(3) . ? C143 N14 1.40(2) . ? C143 C144 1.49(3) . ? C142 S142 1.72(3) . ? C142 H142 0.9500 . ? C144 H14A 0.9800 . ? C144 H14B 0.9800 . ? C144 H14C 0.9800 . ? C211 N21 1.34(2) . ? C211 S212 1.708(18) . ? C211 S211 1.725(17) . ? C213 C212 1.37(3) . ? C213 N21 1.43(2) . ? C213 C214 1.50(3) . ? C212 S212 1.63(2) . ? C212 H212 0.9500 . ? C214 H21A 0.9800 . ? C214 H21B 0.9800 . ? C214 H21C 0.9800 . ? C241 N24 1.33(2) . ? C241 S241 1.710(19) . ? C241 S242 1.744(17) . ? C243 C242 1.33(3) . ? C243 N24 1.41(2) . ? C243 C244 1.57(3) . ? C242 S242 1.74(2) . ? C242 H242 0.9500 . ? C244 H24A 0.9800 . ? C244 H24B 0.9800 . ? C244 H24C 0.9800 . ? C231 N23 1.30(2) . ? C231 S231 1.696(17) . ? C231 S232 1.753(17) . ? C232 C233 1.33(2) . ? C232 S232 1.71(2) . ? C232 H232 0.9500 . ? C233 N23 1.42(2) . ? C233 C234 1.46(2) . ? C234 H23A 0.9800 . ? C234 H23B 0.9800 . ? C234 H23C 0.9800 . ? C221 N22 1.37(2) . ? C221 S222 1.709(17) . ? C221 S221 1.730(16) . ? C222 C223 1.36(3) . ? C222 S222 1.69(2) . ? C222 H222 0.9500 . ? C223 N22 1.36(2) . ? C223 C224 1.44(2) . ? C224 H22A 0.9800 . ? C224 H22B 0.9800 . ? C224 H22C 0.9800 . ? Au11 N12 2.071(13) . ? Au11 S111 2.260(4) . ? Au11 Au12 2.9899(9) . ? Au11 Au14 3.0175(8) . ? Au12 N13 2.067(12) . ? Au12 S121 2.257(4) . ? Au12 Au13 3.0962(8) . ? Au13 N14 2.061(12) . ? Au13 S131 2.258(4) . ? Au13 Au14 3.0103(9) . ? Au14 N11 2.067(12) . ? Au14 S141 2.258(4) . ? Au21 N22 2.046(13) . ? Au21 S211 2.250(5) . ? Au21 Au22 3.0011(9) . ? Au21 Au24 3.0796(9) . ? Au24 N21 2.028(13) . ? Au24 S241 2.264(5) . ? Au24 Au23 2.9838(9) . ? Au23 N24 2.039(13) . ? Au23 S231 2.264(5) . ? Au23 Au22 3.0080(9) . ? Au22 N23 2.083(12) . ? Au22 S221 2.259(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 C111 S111 128.9(12) . . ? N11 C111 S112 112.1(11) . . ? S111 C111 S112 118.9(8) . . ? C112 C113 N11 112.5(15) . . ? C112 C113 C114 127.8(15) . . ? N11 C113 C114 119.7(14) . . ? C113 C112 S112 111.7(13) . . ? C113 C112 H112 124.1 . . ? S112 C112 H112 124.1 . . ? C113 C114 H11A 109.5 . . ? C113 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C113 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? N12 C121 S122 113.7(14) . . ? N12 C121 S121 127.9(13) . . ? S122 C121 S121 118.2(13) . . ? C122 C123 N12 114.0(19) . . ? C122 C123 C124 124.6(18) . . ? N12 C123 C124 121.4(17) . . ? C123 C122 S122 110.9(15) . . ? C123 C122 H122 124.5 . . ? S122 C122 H122 124.5 . . ? C123 C124 H12A 109.5 . . ? C123 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? C123 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? N13 C131 S131 129.6(12) . . ? N13 C131 S132 111.1(11) . . ? S131 C131 S132 119.2(9) . . ? C132 C133 N13 111.2(15) . . ? C132 C133 C134 127.6(16) . . ? N13 C133 C134 121.2(16) . . ? C133 C132 S132 111.3(13) . . ? C133 C132 H132 124.3 . . ? S132 C132 H132 124.3 . . ? C133 C134 H13A 109.5 . . ? C133 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C133 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? N14 C141 S141 128.8(12) . . ? N14 C141 S142 112.8(11) . . ? S141 C141 S142 118.4(10) . . ? C142 C143 N14 112.0(19) . . ? C142 C143 C144 126.3(18) . . ? N14 C143 C144 121.6(17) . . ? C143 C142 S142 111.3(15) . . ? C143 C142 H142 124.3 . . ? S142 C142 H142 124.3 . . ? C143 C144 H14A 109.5 . . ? C143 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C143 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? N21 C211 S212 113.4(13) . . ? N21 C211 S211 127.5(13) . . ? S212 C211 S211 119.0(10) . . ? C212 C213 N21 110.5(15) . . ? C212 C213 C214 129.0(19) . . ? N21 C213 C214 120.4(18) . . ? C213 C212 S212 114.5(15) . . ? C213 C212 H212 122.8 . . ? S212 C212 H212 122.8 . . ? C213 C214 H21A 109.5 . . ? C213 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C213 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? N24 C241 S241 130.7(13) . . ? N24 C241 S242 112.8(13) . . ? S241 C241 S242 116.5(11) . . ? C242 C243 N24 114(2) . . ? C242 C243 C244 128.5(19) . . ? N24 C243 C244 117.5(18) . . ? C243 C242 S242 111.9(16) . . ? C243 C242 H242 124.0 . . ? S242 C242 H242 124.0 . . ? C243 C244 H24A 109.5 . . ? C243 C244 H24B 109.5 . . ? H24A C244 H24B 109.5 . . ? C243 C244 H24C 109.5 . . ? H24A C244 H24C 109.5 . . ? H24B C244 H24C 109.5 . . ? N23 C231 S231 131.6(13) . . ? N23 C231 S232 110.8(12) . . ? S231 C231 S232 117.7(9) . . ? C233 C232 S232 114.4(14) . . ? C233 C232 H232 122.8 . . ? S232 C232 H232 122.8 . . ? C232 C233 N23 109.8(16) . . ? C232 C233 C234 128.7(18) . . ? N23 C233 C234 121.4(16) . . ? C233 C234 H23A 109.5 . . ? C233 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C233 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? N22 C221 S222 111.7(11) . . ? N22 C221 S221 128.0(13) . . ? S222 C221 S221 120.2(10) . . ? C223 C222 S222 112.1(16) . . ? C223 C222 H222 123.9 . . ? S222 C222 H222 123.9 . . ? N22 C223 C222 113.4(17) . . ? N22 C223 C224 122.0(16) . . ? C222 C223 C224 124.6(18) . . ? C223 C224 H22A 109.5 . . ? C223 C224 H22B 109.5 . . ? H22A C224 H22B 109.5 . . ? C223 C224 H22C 109.5 . . ? H22A C224 H22C 109.5 . . ? H22B C224 H22C 109.5 . . ? N12 Au11 S111 168.8(4) . . ? N12 Au11 Au12 85.2(4) . . ? S111 Au11 Au12 100.60(14) . . ? N12 Au11 Au14 105.9(4) . . ? S111 Au11 Au14 84.18(11) . . ? Au12 Au11 Au14 86.42(2) . . ? N13 Au12 S121 167.6(4) . . ? N13 Au12 Au11 105.9(4) . . ? S121 Au12 Au11 84.57(12) . . ? N13 Au12 Au13 84.2(4) . . ? S121 Au12 Au13 103.14(13) . . ? Au11 Au12 Au13 87.19(2) . . ? N14 Au13 S131 170.4(4) . . ? N14 Au13 Au14 83.6(4) . . ? S131 Au13 Au14 102.09(12) . . ? N14 Au13 Au12 105.8(4) . . ? S131 Au13 Au12 82.60(10) . . ? Au14 Au13 Au12 84.68(2) . . ? N11 Au14 S141 166.2(4) . . ? N11 Au14 Au13 106.9(4) . . ? S141 Au14 Au13 85.19(12) . . ? N11 Au14 Au11 85.0(3) . . ? S141 Au14 Au11 102.22(12) . . ? Au13 Au14 Au11 88.27(2) . . ? N22 Au21 S211 173.1(4) . . ? N22 Au21 Au22 86.0(4) . . ? S211 Au21 Au22 98.66(13) . . ? N22 Au21 Au24 101.9(3) . . ? S211 Au21 Au24 83.80(13) . . ? Au22 Au21 Au24 84.10(2) . . ? N21 Au24 S241 169.4(4) . . ? N21 Au24 Au23 102.4(3) . . ? S241 Au24 Au23 86.00(13) . . ? N21 Au24 Au21 84.1(4) . . ? S241 Au24 Au21 102.55(14) . . ? Au23 Au24 Au21 89.24(2) . . ? N24 Au23 S231 168.0(4) . . ? N24 Au23 Au24 84.9(4) . . ? S231 Au23 Au24 101.62(13) . . ? N24 Au23 Au22 105.4(3) . . ? S231 Au23 Au22 85.30(12) . . ? Au24 Au23 Au22 85.66(2) . . ? N23 Au22 S221 164.9(4) . . ? N23 Au22 Au21 109.2(3) . . ? S221 Au22 Au21 84.57(12) . . ? N23 Au22 Au23 85.2(4) . . ? S221 Au22 Au23 101.26(15) . . ? Au21 Au22 Au23 90.28(2) . . ? C111 N11 C113 113.4(13) . . ? C111 N11 Au14 124.4(11) . . ? C113 N11 Au14 121.3(10) . . ? C131 N13 C133 115.1(13) . . ? C131 N13 Au12 123.8(10) . . ? C133 N13 Au12 120.7(11) . . ? C141 N14 C143 113.4(14) . . ? C141 N14 Au13 125.7(10) . . ? C143 N14 Au13 120.8(12) . . ? C211 N21 C213 110.6(14) . . ? C211 N21 Au24 126.8(11) . . ? C213 N21 Au24 122.7(11) . . ? C241 N24 C243 111.9(15) . . ? C241 N24 Au23 124.3(11) . . ? C243 N24 Au23 123.3(13) . . ? C231 N23 C233 115.6(14) . . ? C231 N23 Au22 123.4(11) . . ? C233 N23 Au22 119.8(11) . . ? C223 N22 C221 112.2(14) . . ? C223 N22 Au21 124.0(12) . . ? C221 N22 Au21 123.6(11) . . ? C121 N12 C123 111.8(14) . . ? C121 N12 Au11 124.1(12) . . ? C123 N12 Au11 124.0(12) . . ? C111 S111 Au11 109.4(5) . . ? C112 S112 C111 90.3(8) . . ? C121 S121 Au12 107.4(6) . . ? C121 S122 C122 89.5(10) . . ? C131 S131 Au13 109.5(5) . . ? C132 S132 C131 91.2(8) . . ? C141 S141 Au14 107.5(6) . . ? C142 S142 C141 90.4(9) . . ? C211 S211 Au21 108.6(6) . . ? C212 S212 C211 90.9(9) . . ? C241 S241 Au24 106.8(6) . . ? C242 S242 C241 89.3(9) . . ? C231 S231 Au23 109.2(6) . . ? C232 S232 C231 89.4(8) . . ? C221 S221 Au22 108.1(6) . . ? C222 S222 C221 90.5(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Au11 Au14 N11 C111 -22.1(12) . . . . ? Au14 Au11 S111 C111 -22.6(6) . . . . ? Au11 Au14 N11 S111 -17.8(3) . . . . ? Au12 Au11 N12 C121 19.7(12) . . . . ? Au11 Au12 S121 C121 27.9(6) . . . . ? Au12 Au11 N12 S121 19.6(3) . . . . ? Au13 Au12 N13 C131 -21.1(13) . . . . ? Au12 Au13 S131 C131 -26.7(6) . . . . ? Au13 Au12 N13 S131 -19.3(3) . . . . ? Au14 Au13 N14 C141 20.7(13) . . . . ? Au13 Au14 S141 C141 25.1(6) . . . . ? Au14 Au13 N14 S141 18.6(3) . . . . ? Au21 Au24 N21 C211 -14.9(12) . . . . ? Au24 Au21 S211 C211 -26.2(6) . . . . ? Au21 Au24 N21 S211 -17.2(3) . . . . ? Au22 Au21 N22 C221 18.6(12) . . . . ? Au21 Au22 S221 C221 26.4(6) . . . . ? Au22 Au21 N22 S221 18.5(3) . . . . ? Au23 Au22 N23 C231 -19.6(12) . . . . ? Au22 Au23 S231 C231 -17.2(6) . . . . ? Au23 Au22 N23 S231 -14.6(3) . . . . ? Au24 Au23 N24 C241 20.7(11) . . . . ? Au23 Au24 S241 C241 21.4(6) . . . . ? Au24 Au23 N24 S241 17.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.481 _refine_diff_density_min -3.515 _refine_diff_density_rms 0.377 #===END